CN113122895B - A method for cathode parallel regulation of electrochemically induced mineral deposition rate - Google Patents
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- HJPBEXZMTWFZHY-UHFFFAOYSA-N [Ti].[Ru].[Ir] Chemical compound [Ti].[Ru].[Ir] HJPBEXZMTWFZHY-UHFFFAOYSA-N 0.000 claims description 5
- 230000001965 increasing effect Effects 0.000 claims description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001424 calcium ion Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
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- C25D9/00—Electrolytic coating other than with metals
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
本发明涉及一种阴极并联调控电化学诱导矿物沉积速率的方法，包括以下步骤：(1)构建由阴极、阳极和电解质溶液组成的电极体系，其中，阴极设有并联的两个，在两个阴极的外侧分别固定有一阳极；(2)调整两个阴极之间的距离，即实现阴极表面矿物沉积速率的调控。与现有技术相比，本发明在保持阴极电流密度、无机矿物自身性质不变的前提下，实现矿物生长速率的有效调控，为该技术在建筑材料领域中的应用奠定坚实的基础。
The present invention relates to a method for regulating and controlling electrochemically induced mineral deposition rate in parallel with cathodes. An anode is respectively fixed on the outer side of the cathode; (2) the distance between the two cathodes is adjusted, that is, the regulation of the mineral deposition rate on the cathode surface is realized. Compared with the prior art, the present invention realizes effective regulation of mineral growth rate on the premise of keeping the cathode current density and the properties of inorganic minerals unchanged, laying a solid foundation for the application of the technology in the field of building materials.
Description
技术领域technical field
本发明属于电化学沉积技术领域，涉及一种阴极并联调控电化学诱导矿物沉积速率的方法。The invention belongs to the technical field of electrochemical deposition, and relates to a method for controlling the deposition rate of electrochemically induced minerals in parallel with cathodes.
背景技术Background technique
电化学沉积技术在金属、纳米及薄膜领域已有广泛的应用，沉积物的导电性与沉积的持续性、均匀性密切相关。因此，该技术在非导电无机矿物领域的发展并不具备优势。目前，电沉积无机矿物技术也仅主要应用于混凝土裂缝修补、阴极保护等领域。上世纪70年代，Wolf H.Hilbertz首次提出利用电化学沉积技术在海水中原位制备一种无机矿物建筑材料的技术。近年来，学者们探究了电流密度、阴极材料等参数对电沉积物生长的影响规律；确定了沉积物的主要组成为Mg(OH)2和少量CaCO3；同时对沉积物的力学性能进行研究，确立了这种无机矿物应用于建筑领域的潜力。但矿物的生长速率低是这一技术发展的最大难题。目前，提升沉积物生长速率的主要手段是提高阴极表面电流密度，这种方法仅在一定电流密度范围内有效，且因为阴极表面H2气泡生成速率也随电流密度增加而增大，气泡对沉积物的力学性能具有很大影响，甚至导致沉积物从阴极表面剥落。因此，在不影响阴极表面无机矿物自身性质的前提下，提升沉积物生长速率是目前亟待解决的难题。Electrochemical deposition technology has been widely used in the fields of metals, nanometers and thin films. The conductivity of the deposit is closely related to the continuity and uniformity of the deposition. Therefore, the development of this technology in the field of non-conductive inorganic minerals does not have advantages. At present, electrodeposited inorganic mineral technology is only mainly used in concrete crack repair, cathodic protection and other fields. In the 1970s, Wolf H. Hilbertz first proposed the use of electrochemical deposition technology to prepare an inorganic mineral building material in situ in seawater. In recent years, scholars have explored the influence of current density, cathode material and other parameters on the growth of electrodeposits; determined that the main composition of the deposit is Mg(OH) 2 and a small amount of CaCO 3 ; at the same time, the mechanical properties of the deposit have been studied. , establishing the potential of this inorganic mineral for use in construction. But the low growth rate of minerals is the biggest problem in the development of this technology. At present, the main method to increase the deposition growth rate is to increase the current density on the cathode surface. This method is only effective in a certain current density range, and because the H2 bubble generation rate on the cathode surface also increases with the increase of the current density, the bubbles have no effect on the deposition. The mechanical properties of the material have a great influence, and even lead to the exfoliation of the deposit from the cathode surface. Therefore, without affecting the properties of the inorganic minerals on the cathode surface, it is an urgent problem to improve the sediment growth rate.
发明内容SUMMARY OF THE INVENTION
本发明的目的就是为了提供一种阴极并联调控电化学诱导矿物沉积速率的方法，在不影响沉积矿物自身性质的基础上，有效提升电沉积物原位生长速率，从而为电化学诱导矿物在建筑领域中的应用奠定坚实的基础。The purpose of the present invention is to provide a method for controlling the deposition rate of electrochemically induced minerals in parallel with cathodes, which can effectively improve the in-situ growth rate of electrodeposits without affecting the properties of the deposited minerals, thereby providing a good solution for the electrochemically induced minerals in buildings. The application in the field lays a solid foundation.
本发明的目的可以通过以下技术方案来实现：The object of the present invention can be realized through the following technical solutions:
本发明提供了一种阴极并联调控电化学诱导矿物沉积速率的方法，包括以下步骤：The invention provides a method for cathode parallel regulation of electrochemically induced mineral deposition rate, comprising the following steps:
(1)构建由阴极、阳极和电解质溶液组成的电极体系，其中，阴极设有并联的两个，在两个阴极的外侧分别固定有一阳极；(1) constructing an electrode system consisting of a cathode, an anode and an electrolyte solution, wherein two cathodes are arranged in parallel, and an anode is respectively fixed on the outside of the two cathodes;
(2)调整两个阴极之间的距离，即实现阴极表面矿物沉积速率的调控。(2) Adjust the distance between the two cathodes, that is, to realize the regulation of the mineral deposition rate on the cathode surface.
进一步的，调控过程中，两个阴极之间的距离越小，阴极表面矿物沉积速率提升越大。Further, during the regulation process, the smaller the distance between the two cathodes, the greater the increase in the mineral deposition rate on the cathode surface.
进一步的，两个阴极分别和位于其外侧的阳极平行。Further, the two cathodes are respectively parallel to the anodes located outside of them.
进一步的，两个阴极分别与位于其外侧的阳极的距离相同。Further, the distances between the two cathodes and the anode located outside them are the same.
进一步的，两个阴极之间平行并联，且两个阴极的材料、尺寸均相同。Further, the two cathodes are connected in parallel and in parallel, and the materials and dimensions of the two cathodes are the same.
进一步的，两阴极之间的间距为阴极宽度或直径的6倍以内，具体的，当阴极为片状或网状时，则以其宽度为计量基准，当阴极为棒状或柱状时，则以其直径为计量基准。Further, the distance between the two cathodes is within 6 times of the width or diameter of the cathodes. Specifically, when the cathodes are in the shape of sheets or meshes, the width is used as the measurement basis, and when the cathodes are in the shape of rods or columns, the Its diameter is the measurement benchmark.
进一步的，所述阴极为金属片、金属网或金属棒。Further, the cathode is a metal sheet, a metal mesh or a metal rod.
进一步的，所述阳极为钌铱钛片或铂金片。Further, the anode is a ruthenium iridium titanium sheet or a platinum sheet.
进一步的，所述电解质溶液为包含镁离子和/或钙离子的水溶液。Further, the electrolyte solution is an aqueous solution containing magnesium ions and/or calcium ions.
进一步的，所述阴极和阳极分别与外部电源的负极和正极相连接。Further, the cathode and the anode are respectively connected with the negative electrode and the positive electrode of the external power source.
本发明所涉及的阴极并联提升电化学诱导矿物沉积速率的方法，相比于现有的调控方法，具有如下创新点及优势：通过阴极并联，实现阴极表面OH-浓度叠加，在不改变电流密度的前提下，实现了阴极表面OH-浓度的提升，进而提高了Mg(OH)2等难溶矿物在阴极表面的生成速率。这种方式既避免了电流密度增大对沉积物孔结构的不利影响，又有效缩短了电化学诱导矿物沉积的周期，提升了沉积效率、降低了生产能耗。Compared with the existing control method, the method for increasing the electrochemically induced mineral deposition rate in parallel with the cathodes involved in the present invention has the following innovations and advantages: through the parallel connection of the cathodes, the superposition of the OH - concentration on the cathode surface is realized, and the current density is not changed. Under the premise of , the OH - concentration on the cathode surface is increased, and the generation rate of insoluble minerals such as Mg(OH) 2 on the cathode surface is improved. This method not only avoids the adverse effect of the increase of the current density on the sediment pore structure, but also effectively shortens the period of electrochemically induced mineral deposition, improves the deposition efficiency and reduces the production energy consumption.
附图说明Description of drawings
图1为本发明的阴极并联示意图；Fig. 1 is the cathode parallel schematic diagram of the present invention;
图中标记说明：Description of marks in the figure:
1-外部电源，2-导线，3-一号阳极，4-二号阳极，5-一号阴极，6-二号阴极。1-External power supply, 2-Wire, 3-No.1 anode, 4-No.2 anode, 5-No.1 cathode, 6-No.2 cathode.
图2为并联阴极表面OH-浓度分布、叠加示意图。FIG. 2 is a schematic diagram of the OH − concentration distribution and superposition on the surface of the parallel cathodes.
图3为并联网状阴极及其所得沉积物照片。Figure 3 is a photograph of the parallel networked cathodes and the resulting deposits.
图4为间距0.5cm并联棒状阴极及其所得沉积物照片。Figure 4 is a photograph of parallel rod-shaped cathodes with a spacing of 0.5 cm and the resulting deposits.
图5为间距3.5cm的并联棒状阴极及其所得沉积物照片。Figure 5 is a photograph of parallel rod cathodes with a spacing of 3.5 cm and the resulting deposits.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明进行详细说明。本实施例以本发明技术方案为前提进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. This embodiment is implemented on the premise of the technical solution of the present invention, and provides a detailed implementation manner and a specific operation process, but the protection scope of the present invention is not limited to the following embodiments.
为了在不影响沉积矿物自身性质的基础上，有效提升电沉积物原位生长速率，从而为电化学诱导矿物在建筑领域中的应用奠定坚实的基础，本发明提供了一种阴极并联调控电化学诱导矿物沉积速率的方法，参见图1所示，包括以下步骤：In order to effectively improve the in-situ growth rate of electrodeposits without affecting the properties of the deposited minerals, thereby laying a solid foundation for the application of electrochemically induced minerals in the field of construction, the invention provides a cathode parallel control electrochemical method. The method for inducing mineral deposition rate, shown in Figure 1, includes the following steps:
(1)构建由阴极、阳极和电解质溶液组成的电极体系，其中，阴极设有并联的两个，在两个阴极的外侧分别固定有一阳极；(1) constructing an electrode system consisting of a cathode, an anode and an electrolyte solution, wherein two cathodes are arranged in parallel, and an anode is respectively fixed on the outside of the two cathodes;
(2)调整两个阴极之间的距离，即实现阴极表面矿物沉积速率的调控。(2) Adjust the distance between the two cathodes, that is, to realize the regulation of the mineral deposition rate on the cathode surface.
在一些实施方式中，调控过程中，两个阴极之间的距离越小，阴极表面矿物沉积速率提升越大。In some embodiments, during the regulation process, the smaller the distance between the two cathodes, the greater the increase in the rate of mineral deposition on the cathode surface.
在一些实施方式中，两个阴极分别和位于其外侧的阳极平行。In some embodiments, the two cathodes are respectively parallel to the anode located outside them.
在一些实施方式中，两个阴极分别与位于其外侧的阳极的距离相同。In some embodiments, the two cathodes are each the same distance from the anode located outside them.
在一些实施方式中，两个阴极之间平行并联，且两个阴极的材料、尺寸均相同。In some embodiments, the two cathodes are connected in parallel, and the materials and dimensions of the two cathodes are the same.
在一些实施方式中，两阴极之间的间距为阴极宽度或直径的6倍以内，具体的，当阴极为片状或网状时，则以其宽度为计量基准，当阴极为棒状或柱状时，则以其直径为计量基准。In some embodiments, the distance between the two cathodes is within 6 times of the width or diameter of the cathodes. Specifically, when the cathodes are in the shape of sheets or meshes, the width is used as the measurement basis, and when the cathodes are in the shape of rods or columns , then its diameter is the measurement benchmark.
在一些实施方式中，所述阴极为金属片、金属网或金属棒。In some embodiments, the cathode is a metal sheet, metal mesh or metal rod.
在一些实施方式中，所述阳极为钌铱钛片或铂金片。In some embodiments, the anode is a ruthenium iridium titanium sheet or a platinum sheet.
在一些实施方式中，所述电解质溶液为包含镁离子和/或钙离子的水溶液。In some embodiments, the electrolyte solution is an aqueous solution containing magnesium ions and/or calcium ions.
在一些实施方式中，所述阴极和阳极分别与外部电源的负极和正极相连接。In some embodiments, the cathode and anode are connected to the negative and positive electrodes of an external power source, respectively.
本发明中，本发明中，将两个材料、尺寸相同的阴极分别与外部电源的负极相连接，即阴极平行并联。在电沉积过程中，两个阴极表面均发生水分子还原生成氢气(H2)和氢氧根离子(OH-)的反应。阴极表面生成的OH-向远离阴极表面的方向发生扩散，即阴极表面附近溶液中的OH-以一定浓度梯度存在。而两个阴极之间溶液中的OH-浓度必然相互叠加，叠加后的OH-浓度升高，且与阴极附近Mg2+等金属离子碰撞、结合的几率增加，最终体现为Mg(OH)2等难溶性晶体生长速率的提升。值得注意，阴极并联在提升沉积物生长速率的同时，并没有改变单个阴极表面电流密度，即单个阴极表面H2气泡生成速率并未增大，实现了阴极沉积物自身性质的稳定。In the present invention, in the present invention, two cathodes with the same material and size are respectively connected to the negative electrodes of the external power supply, that is, the cathodes are connected in parallel and in parallel. During the electrodeposition process, the reduction of water molecules to hydrogen (H 2 ) and hydroxide ions (OH - ) occurs on both cathode surfaces. The OH - generated on the cathode surface diffuses away from the cathode surface, that is, the OH - in the solution near the cathode surface exists with a certain concentration gradient. The OH - concentration in the solution between the two cathodes must be superimposed on each other, the superimposed OH - concentration increases, and the probability of collision and combination with metal ions such as Mg 2+ near the cathode increases, which is finally reflected as Mg(OH) 2 and other insoluble crystal growth rates. It is worth noting that the parallel connection of cathodes improves the deposition growth rate without changing the current density on the surface of a single cathode, that is, the generation rate of H bubbles on the surface of a single cathode does not increase, thus achieving the stability of the properties of the cathode deposit itself.
以上各实施方式可以任一单独实施，也可以任意两两组合或更多的组合实施。The above embodiments may be implemented individually, or may be implemented in any two or more combinations.
下面结合具体实施例来对上述实施方式进行更详细的说明。The above embodiments will be described in more detail below with reference to specific embodiments.
一种阴极并联调控电化学诱导矿物沉积速率的方法，阴极及阳极的连接方式参见图1，整个电极体系包括提供电流的外部电源(可以为直流电源)以及输送电流的导线，材料相同、尺寸相同、彼此相互平行并联的一号阴极和二号阴极，分别位于一号阴极和二号阴极外侧的一号阳极和二号阳极，阴极表面OH-离子浓度分布示意图如图2所示，二者存在叠加区域。A method for controlling the rate of electrochemically induced mineral deposition in parallel with cathodes. The connection method of cathode and anode is shown in Figure 1. The entire electrode system includes an external power supply (which can be a DC power supply) that provides current and a wire that transmits current. The materials are the same and the dimensions are the same. , No. 1 cathode and No. 2 cathode which are parallel and parallel to each other, No. 1 anode and No. 2 anode respectively located on the outside of No. 1 cathode and No. 2 cathode, the schematic diagram of the OH - ion concentration distribution on the cathode surface is shown in Figure 2, and the two exist Overlay area.
采用上述方式开展阴极并联调控电化学诱导矿物沉积速率的实验，具体如下述实施例。The above-mentioned method is used to carry out an experiment of controlling the electrochemically induced mineral deposition rate in parallel with cathodes, as described in the following examples.
实施例1：Example 1:
选取浓度为0.15mol/L的MgCl2、0.03mol/L的CaCl2及0.0069mol/L的NaHCO3混合溶液作为电解质溶液；阳极材料选用直径为0.3cm的钌铱钛棒，选用两片6cm*5cm的304不锈钢网(丝径0.5mm，孔径3.8mm)作为阴极，控制阴极和阳极间的距离为4cm，并联的阴极间的距离为1cm，控制电极浸入液面深度为6cm；外部电源选择稳压直流电源，采用恒电流模式，电流大小设置为20mA；每隔24h更换电解质溶液，确保电解质浓度及pH基本保持不变；沉积时间设置为720h。所得沉积产物的平均厚度为10.8mm，相比于单层阴极沉积物厚度增长率为24.14％。A mixed solution of 0.15mol/L MgCl 2 , 0.03 mol/L CaCl 2 and 0.0069 mol/L NaHCO 3 was selected as the electrolyte solution; the anode material was a ruthenium-iridium-titanium rod with a diameter of 0.3cm, and two 6cm* 5cm of 304 stainless steel mesh (wire diameter 0.5mm, aperture 3.8mm) is used as the cathode, the distance between the control cathode and the anode is 4cm, the distance between the parallel cathodes is 1cm, and the control electrode is immersed into the liquid level at a depth of 6cm; the external power supply is selected to be stable. The voltage DC power supply adopts constant current mode, and the current size is set to 20mA; the electrolyte solution is replaced every 24h to ensure that the electrolyte concentration and pH remain basically unchanged; the deposition time is set to 720h. The average thickness of the obtained deposition product was 10.8 mm, and the growth rate was 24.14% compared to the thickness of the single-layer cathode deposit.
实施例2Example 2
选取浓度为0.15mol/L的MgCl2、0.03mol/L的CaCl2及0.0069mol/L的NaHCO3混合溶液作为电解质溶液；阳极材料选用直径为0.3mm的钌铱钛棒，选用两根
对比例3：Comparative Example 3:
与实施例2相比，绝大部分都相同，除了两阴极的间距调整为3.5cm，即阴极直径的7倍。所得沉积产物的平均厚度为1.9mm。Compared with Example 2, most of them are the same, except that the distance between the two cathodes is adjusted to 3.5 cm, which is 7 times the diameter of the cathodes. The average thickness of the resulting deposited product was 1.9 mm.
依据实施案例1和2及对比例3所得沉积矿物照片如图3(其中，图3a为并联网状阴极的图片，图3b则为所得沉积物的照片)、图4(其中，图4a为并联棒状阴极的图片，图4b为所得沉积物的图片)和图5(其中，图5a为并联棒状阴极的图片，图5b为所得沉积物的图片)所示。表1列出了上述实施例1和实施例2阴极并联所得沉积物的平均厚度，并与单阴极所得沉积物厚度(即分别与实施例1、2比较，除去采用单一的阴极与阳极外，其余条件均不变的对比例1和对比例2)进行对比。同时，列出了上述实施例2与对比例3阴极并联所得沉积物的平均厚度(即与实施例2比较，除去采用两阴极间距扩大至阴极直径的7倍外，其余条件均不变)进行对比。对于双层网状阴极，沉积物厚度增长率为24.14％；对于棒状阴极，阴极并联所得沉积物厚度较单阴极增长了26.32％。对于棒状阴极，两阴极间距为0.5cm(即阴极间距的1倍)所得沉积物厚度较间距为3.5cm(即阴极间距的7倍)的两阴极增长了26.32％。此外，从以上两个具体实施案例可以发现，阴极并联对沉积矿物厚度增长速率具有明显促进作用，增长率达25％左右。通过调整并联阴极之间的距离可以进一步调控沉积物的生长速率。同时，对比实施案例2与对比例3可以发现，两阴极间距增大至阴极直径的6倍以上后，阴极并联对沉积矿物厚度增长速率的促进作用消失。The photos of sedimentary minerals obtained according to Examples 1 and 2 and Comparative Example 3 are shown in Figure 3 (wherein, Figure 3a is a photo of the parallel-connected cathode, and Figure 3b is a photo of the obtained sediment), Figure 4 (wherein, Figure 4a is a parallel connection. Pictures of rod cathodes, Figure 4b is a picture of the resulting deposit) and Figure 5 (wherein Figure 5a is a picture of a parallel rod cathode and Figure 5b is a picture of the resulting deposit). Table 1 lists the average thickness of the deposits obtained in the above-mentioned Example 1 and Example 2 in parallel with the cathodes, and the thickness of the deposits obtained with a single cathode (that is, compared with Examples 1 and 2 respectively, except that a single cathode and anode are used, Comparative example 1 and comparative example 2) with the other conditions unchanged are compared. At the same time, the average thickness of the deposits obtained in parallel with the cathodes of Example 2 and Comparative Example 3 (that is, compared with Example 2, except that the distance between the two cathodes is expanded to 7 times the diameter of the cathodes, the rest of the conditions are unchanged). Compared. For the double-layer mesh cathode, the growth rate of the deposit thickness is 24.14%; for the rod-shaped cathode, the thickness of the deposit obtained in parallel with the cathode increases by 26.32% compared with the single cathode. For rod-shaped cathodes, the thickness of the deposit obtained with a spacing of 0.5 cm (ie, 1 times the cathode spacing) increased by 26.32% compared with two cathodes with a spacing of 3.5 cm (ie, 7 times the cathode spacing). In addition, from the above two specific implementation cases, it can be found that the parallel connection of cathodes can significantly promote the growth rate of the thickness of sedimentary minerals, and the growth rate is about 25%. The growth rate of the deposit can be further regulated by adjusting the distance between the parallel cathodes. At the same time, comparing Example 2 and Comparative Example 3, it can be found that when the distance between the two cathodes is increased to more than 6 times the diameter of the cathode, the promoting effect of the parallel connection of the cathodes on the growth rate of the deposited mineral thickness disappears.
表1Table 1
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。The foregoing description of the embodiments is provided to facilitate understanding and use of the invention by those of ordinary skill in the art. It will be apparent to those skilled in the art that various modifications to these embodiments can be readily made, and the generic principles described herein can be applied to other embodiments without inventive step. Therefore, the present invention is not limited to the above-mentioned embodiments, and improvements and modifications made by those skilled in the art according to the disclosure of the present invention without departing from the scope of the present invention should all fall within the protection scope of the present invention.
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